CN101702376B - Method used for preparing titanium dioxide film of electrode of solar battery - Google Patents
Method used for preparing titanium dioxide film of electrode of solar battery Download PDFInfo
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- CN101702376B CN101702376B CN 200910218649 CN200910218649A CN101702376B CN 101702376 B CN101702376 B CN 101702376B CN 200910218649 CN200910218649 CN 200910218649 CN 200910218649 A CN200910218649 A CN 200910218649A CN 101702376 B CN101702376 B CN 101702376B
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Abstract
The invention relates to a method used for preparing a titanium dioxide film of an electrode of a solar battery. Species with different functions are assembled on a plane substrate layer by layer by an electrostatic layer-by-layer self-assembly technology through an electrostatic or covalent bonding function, and a plurality of layers of orderly films are constructed within the range of a nano dimension. The invention can prepare the titanium dioxide nano film with smooth and uniform surface, large clearance rate, large specific surface area and accurate and controllable thickness, and the prepared titanium dioxide film has higher mechanical strength, uniform clearance distribution, large specific surface area, no cracking, no desquamation and accurate regulation and control of the thickness and can improve the stability of the battery, increase the adsorption quantity of dye and enhance the efficiency of light absorption.
Description
Technical field
The invention belongs to the DSSC technical field, relate to and a kind ofly be used for the method for the titanium deoxid film of working electrode of solar cell, be applied to DSSC with static self assembly layer by layer preparation.
Background technology
Last century, the nineties was with afterwards, DSSC has caused people's extensive interest, and with respect to normally used crystal silicon solar energy battery, DSSC is with low cost, manufacture craft is simple to operation, having a high potential at solar energy development and aspect utilizing.
DSSC mainly constitutes by work electrode, dielectric substrate with to electrode, and wherein the character of titanium deoxid film work electrode is the key factor that influences the electricity conversion of battery.At present, the relevant method for preparing the nano-tube film electrode is mainly coating process, and silk screen print method etc., these methods still can't effectively be regulated and control TiO in the nanoscale scope and on the molecular structure level
2The degree of order and film thickness, and orderly TiO
2Array has been proved photoelectric current and the optoelectronic transformation efficiency that helps to improve battery.
Summary of the invention:
The object of the present invention is to provide a kind of utilize static layer by layer self-assembling method under temperate condition, prepare the method for the controlled ordered nano titanium deoxid film of nanometer, the film of preparation has higher mechanical strength, the space is evenly distributed, specific area is big, do not ftracture, do not peel off, but thickness accuracy controlling, can improve stability test, increase the dyestuff adsorbance, improve extinction efficient.
Objects of the present invention are achieved through the following technical solutions, and a kind of preparation method who is used for the titanium deoxid film of electrode of solar battery may further comprise the steps:
(1) preparation TiO
2Suspension
With titanium dioxide and pH value is the Na of 8-12
2CO
3-NaHCO
3Cushioning liquid is configured to the suspension that concentration is 2wt%, earlier titanium dioxide being ground the back mixes with cushioning liquid, ultrasonic again dispersion 30 minutes, regulate titanium dioxide pH value on demand, make titanium dioxide granule be electropositive, the pH value is lower than the titanium dioxide isopotential point, perhaps makes titanium dioxide granule be elecrtonegativity, the pH value is higher than the titanium dioxide isopotential point, does not stop in the whole process to stir;
(2) preparation polyelectrolyte solution
Polyelectrolyte is mixed with the Na of 0.1-3g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value makes polyelectrolyte solution opposite with the tio_2 suspension band electrical;
(3) preparation titanium deoxid film
On electro-conductive glass,, prepare the titanium dioxide work electrode with electrostatic layer self-assembling method absorption titanium dioxide layer; The electro-conductive glass substrate of cleaning is immersed 1-10min in the tio_2 suspension of step (1) preparation, make that charged titanium dioxide nano-particle fully is adsorbed in the electro-conductive glass substrate by the electrostatic interaction individual layer in the suspension, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step (2) preparation again, make the polyelectrolyte molecules of being with in the solution with the titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the flush away polyelectrolyte of having more than needed, dry up, finish the self assembly of one deck static;
(4) operation of repeating step (3) installs to titanium dioxide and polyelectrolyte alternate group in the electro-conductive glass substrate, makes titanium deoxid film, up to the thickness that obtains setting;
(5) calcining
The titanium deoxid film of step (3), (4) preparation is calcined 20min-120min down at 300-800 ℃, make nano-titanium dioxide film.
Further technical scheme is, the polyelectrolyte and the titanium dioxide of oppositely charged is contained in the electro-conductive glass substrate by Electrostatic Absorption power alternate group.
Further technical scheme is, the number of plies of electrostatic layer self assembly is 40-200, and the thickness of film is 4-20 μ m.
Further technical scheme is, used polyelectrolyte is a diallyl dimethyl ammoniumchloride, poly--(4-Sodium styrene sulfonate), a kind of in poly-hydroxide propylene ammonia or the polyacrylic acid.
Further technical scheme is that used titanium dioxide is titania nanoparticles, titania nanotube, titanium dioxide nano-rod or titanium dioxide nano thread in the electrode.
The present invention utilizes the electrostatic layer self-assembling technique that the difference in functionality species are assembled on the planar substrates by static or covalent bonding active layer, and makes up the multilayer order film in the nanoscale scope.The titanium deoxid film that utilizes the present invention to prepare has the characteristic of various dimensions such as geometry, size, wall thickness, duct, composition, and these modulus fully can with corresponding one by one design of required function material or the reaction of carrying out and finely regulating.The present invention can prepare that surfacing is even, voidage is big, specific area is big, the accurate controlled titanium dioxide nano-film of thickness, the titanium deoxid film of preparation has higher mechanical strength, the space is evenly distributed, specific area is big, do not ftracture, do not peel off, but the thickness accuracy controlling can be improved stability test, increases the dyestuff adsorbance, improve extinction efficient, be used for DSSC.
Description of drawings
Fig. 1 is with the SEM photo of the resulting titania nanoparticles film of preparation method provided by the invention behind 550 ℃ of sintering;
Fig. 2 is with the SEM photo of the resulting titanic oxide nano tube thin-film of preparation method provided by the invention behind 550 ℃ of sintering.
Preferred forms:
A kind of preparation method who is used for the titanium deoxid film of electrode of solar battery is characterized in that, may further comprise the steps:
(1) preparation TiO
2Suspension
With titanium dioxide and pH value is the Na of 8-12
2CO
3-NaHCO
3Cushioning liquid is configured to the suspension that concentration is 2wt%, earlier titanium dioxide being ground the back mixes with cushioning liquid, ultrasonic again dispersion 30 minutes, regulate titanium dioxide pH value on demand, make titanium dioxide granule be electropositive, the pH value is lower than the titanium dioxide isopotential point, perhaps makes titanium dioxide granule be elecrtonegativity, the pH value is higher than the titanium dioxide isopotential point, does not stop in the whole process to stir;
(2) preparation polyelectrolyte solution
Polyelectrolyte is mixed with the Na of 0.1-3g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value makes polyelectrolyte solution opposite with the tio_2 suspension band electrical;
(3) preparation titanium deoxid film
On electro-conductive glass,, prepare the titanium dioxide work electrode with electrostatic layer self-assembling method absorption titanium dioxide layer; The electro-conductive glass substrate of cleaning is immersed 1-10min in the tio_2 suspension of step (1) preparation, make that charged titanium dioxide nano-particle fully is adsorbed in the electro-conductive glass substrate by the electrostatic interaction individual layer in the suspension, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step (2) preparation again, make the polyelectrolyte molecules of being with in the solution with the titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the flush away polyelectrolyte of having more than needed, dry up, finish the self assembly of one deck static;
(4) operation of repeating step (3) installs to titanium dioxide and polyelectrolyte alternate group in the electro-conductive glass substrate, makes titanium deoxid film, up to the thickness that obtains setting;
(5) calcining
The titanium deoxid film of step (3), (4) preparation is calcined 20min-120min down at 300-800 ℃, make nano-titanium dioxide film.
Used polyelectrolyte is diallyl dimethyl ammoniumchloride, poly--(4-Sodium styrene sulfonate), poly-hydroxide propylene ammonia or polyacrylic acid.
Polyelectrolyte and titanium dioxide with oppositely charged in above-mentioned steps (3), (4) are contained in the electro-conductive glass substrate by Electrostatic Absorption power alternate group.The number of plies of electrostatic layer self assembly is 40-200, and the thickness of film is 4-20 μ m.
Used titanium dioxide is titania nanoparticles, titania nanotube, titanium dioxide nano-rod or titanium dioxide nano thread in the electrode.
The invention will be further described below by embodiment:
Embodiment 1
(1) preparation TiO
2Suspension
It is 10 Na that titania nanoparticles is added a small amount of pH value
2CO
3-NaHCO
3After cushioning liquid grinds, add an amount of pH value again and be 10 Na
2CO
3-NaHCO
3Cushioning liquid, being mixed with concentration is 2wt% suspension, mixes, ultrasonic again dispersion 30 minutes, regulating titanium dioxide pH value is 10, makes titanium dioxide granule be elecrtonegativity;
(2) preparation polyelectrolyte solution
The poly-hydroxide propylene ammonia (PAH) of polyelectrolyte is mixed with the Na2CO of 1g/L
3-NaHCO
3Cushioning liquid, regulator solution pH value is 9, makes polyelectrolyte solution and tio_2 suspension oppositely charged, promptly is electropositive;
(3) preparation titanium deoxid film
The electro-conductive glass substrate of cleaning is immersed 5min in the tio_2 suspension of step (1) preparation, electronegative titanium dioxide nano-particle in the suspension fully is adsorbed in the electro-conductive glass substrate by electrostatic interaction, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step 2 preparation again, make the band in the solution and the polyelectrolyte molecules of titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the poly-hydroxide propylene ammonia (PAH) of flush away polyelectrolyte more than needed, dry up, finish the self assembly of one deck static;
(4) operation in the repeating step 3, titanium dioxide granule and the poly-hydroxide propylene ammonia (PAH) of polyelectrolyte are installed in the electro-conductive glass substrate by Electrostatic Absorption power alternate group, repeat number of assembling steps 40 times, the titania nanoparticles film number of plies that makes is 40, the thickness of film is 4 μ m, as shown in Figure 1.
(5) calcining
The titanium deoxid film of step (3), (4) preparation is calcined 60min down at 500 ℃, make nano-titanium dioxide film.
Embodiment 2
(1) preparation TiO
2Suspension
It is 10 Na that titania nanotube is added a small amount of pH value
2CO
3-NaHCO
3After cushioning liquid grinds, add the Na of an amount of pH value again for 8-12
2CO
3-NaHCO
3Cushioning liquid, being mixed with concentration is 2wt% suspension, mixes, ultrasonic again dispersion 30 minutes, regulating titanium dioxide pH value is 10, makes titanium dioxide granule be elecrtonegativity.
(2) preparation polyelectrolyte solution
Polyelectrolyte diallyl dimethyl ammoniumchloride (PDAC) is mixed with the Na of 1g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value is 6, makes polyelectrolyte solution and tio_2 suspension oppositely charged, promptly is electropositive.
(3) preparation titanium deoxid film
The electro-conductive glass substrate of cleaning is immersed 5min in the tio_2 suspension of step (1) preparation, electronegative titania nanotube in the suspension fully is adsorbed in the electro-conductive glass substrate by electrostatic interaction, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step (2) preparation again, make the band in the solution and the polyelectrolyte molecules of titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the flush away polyelectrolyte diallyl dimethyl ammoniumchloride (PDAC) of having more than needed, dry up, finish the self assembly of one deck static.
(4) operation in the repeating step 3, titanium dioxide pipe and polyelectrolyte diallyl dimethyl ammoniumchloride (PDAC) are installed in the electro-conductive glass substrate by Electrostatic Absorption power alternate group, repeat number of assembling steps 100 times, the titanic oxide nano tube thin-film surface topography that makes as shown in Figure 2, the number of plies is 100, and the thickness of film is 10 μ m.
(5) calcining
The titanium deoxid film of step (3), (4) preparation is calcined 60min down at 550 ℃, make nano titanium oxide pipe film.
Embodiment 3
(1) preparation TiO
2Suspension
It is after 4 cushioning liquid grinds, to add an amount of buffer salt solution of the same race again that titania nanoparticles is added a small amount of pH value, and making concentration is 2wt% suspension, mix, ultrasonic again dispersion 30 minutes, regulating titanium dioxide pH value again is 4, titanium dioxide granule is electropositive.
(2) preparation polyelectrolyte solution
With polyelectrolyte poly--(4-Sodium styrene sulfonate) (PSS) be mixed with the Na of 1g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value is 6, makes polyelectrolyte solution and tio_2 suspension oppositely charged, promptly is elecrtonegativity.
(3) preparation titanium deoxid film
The electro-conductive glass substrate of cleaning is immersed 5min in the tio_2 suspension of step (1) preparation, positively charged titanium dioxide nano-particle in the suspension fully is adsorbed in the electro-conductive glass substrate by electrostatic interaction, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step 2 preparation again, make the band in the solution and the polyelectrolyte molecules of titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, flush away polyelectrolyte more than needed is poly--(4-Sodium styrene sulfonate) (PSS), dry up, finish the self assembly of one deck static.
(4) operation in the repeating step 3, with titanium dioxide granule and polyelectrolyte poly--(4-Sodium styrene sulfonate) (PSS) install in the electro-conductive glass substrate by Electrostatic Absorption power alternate group, repeat number of assembling steps 150 times, making the number of plies is 150, and thickness is the titanium dioxide granule film of 15 μ m.
(5) calcining
The titanium deoxid film of the 3rd step preparation is calcined 60min down at 500 ℃, make nano-titanium dioxide film.
Embodiment 4
(1) preparation TiO
2Suspension
It is after 4 cushioning liquid grinds, to add an amount of buffer salt solution of the same race again that titania nanoparticles is added a small amount of pH value, and making concentration is 2wt% suspension, mix, ultrasonic again dispersion 30 minutes, regulating titanium dioxide pH value again is 4, titanium dioxide granule is electropositive.
(2) preparation polyelectrolyte solution
Polyelectrolyte polyacrylic acid (PAA) is mixed with the Na of 1g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value is 2.5, makes polyelectrolyte solution and tio_2 suspension oppositely charged, promptly is elecrtonegativity.
(3) preparation titanium deoxid film
The electro-conductive glass substrate of cleaning is immersed 5min in the tio_2 suspension of step (1) preparation, positively charged titanium dioxide nano-particle in the suspension fully is adsorbed in the electro-conductive glass substrate by electrostatic interaction, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step 2 preparation again, make the band in the solution and the polyelectrolyte molecules of titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the flush away polyelectrolyte polyacrylic acid (PAA) of having more than needed, dry up, finish the self assembly of one deck static.
(4) operation in the repeating step 3 installs to titanium dioxide granule and polyelectrolyte PAA in the electro-conductive glass substrate by Electrostatic Absorption power alternate group, repeats number of assembling steps 200 times, and making the number of plies is 200, and thickness is the titanium dioxide granule film of 20 μ m.
(5) calcining
The titanium deoxid film of the 3rd step preparation is calcined 60min down at 500 ℃, make nano-titanium dioxide film.
Claims (5)
1. a preparation method who is used for the titanium deoxid film of electrode of solar battery is characterized in that, may further comprise the steps:
(1) preparation TiO
2Suspension
With titanium dioxide and pH value is the Na of 8-12
2CO
3-NaHCO
3Cushioning liquid is configured to 2wt% suspension, earlier titanium dioxide being ground the back mixes with cushioning liquid, ultrasonic again dispersion 30 minutes, regulate titanium dioxide pH value on demand, make titanium dioxide granule be electropositive, the pH value is lower than the titanium dioxide isopotential point, perhaps makes titanium dioxide granule be elecrtonegativity, the pH value is higher than the titanium dioxide isopotential point, does not stop in the whole process to stir;
(2) preparation polyelectrolyte solution
Polyelectrolyte is mixed with the Na of 0.1-3g/L
2CO
3-NaHCO
3Cushioning liquid, regulator solution pH value makes polyelectrolyte solution opposite with the tio_2 suspension band electrical;
(3) preparation titanium deoxid film
On electro-conductive glass,, prepare the titanium dioxide work electrode with electrostatic layer self-assembling method absorption titanium dioxide layer; The electro-conductive glass substrate of cleaning is immersed 1-10min in the tio_2 suspension of step (1) preparation, make that charged titanium dioxide nano-particle fully is adsorbed in the electro-conductive glass substrate by the electrostatic interaction individual layer in the suspension, take out back washed with de-ionized water 3 times, the flush away titanium dioxide of having more than needed, dry up, immerse the polyelectrolyte solution 5min of step (2) preparation again, make the polyelectrolyte molecules of being with in the solution with the titanium dioxide opposite charges fully be adsorbed on the titanium deoxid film, take out back washed with de-ionized water 3 times, the flush away polyelectrolyte of having more than needed, dry up, finish the self assembly of one deck static;
(4) operation of repeating step (3) installs to titanium dioxide and polyelectrolyte alternate group in the electro-conductive glass substrate, makes titanium deoxid film, up to the thickness that obtains setting;
(5) calcining
The titanium deoxid film of step (3), (4) preparation is calcined 20min-120min down at 300-800 ℃, make nano-titanium dioxide film.
2. the preparation method who is used for the titanium deoxid film of electrode of solar battery as claimed in claim 1, it is characterized in that: in the described step (4), the polyelectrolyte and the titanium dioxide of oppositely charged is contained in the electro-conductive glass substrate by Electrostatic Absorption power alternate group.
3. the preparation method who is used for the titanium deoxid film of electrode of solar battery as claimed in claim 1 is characterized in that: the number of plies of electrostatic layer self assembly is 40-200, and the thickness of film is 4-20 μ m.
4. the preparation method who is used for the titanium deoxid film of electrode of solar battery as claimed in claim 1, it is characterized in that: used polyelectrolyte is a diallyl dimethyl ammoniumchloride, poly--(4-Sodium styrene sulfonate), a kind of in poly-hydroxide propylene ammonia or the polyacrylic acid.
5. the preparation method who is used for the titanium deoxid film of electrode of solar battery as claimed in claim 1 is characterized in that: used titanium dioxide is titania nanoparticles, titania nanotube, titanium dioxide nano-rod or titanium dioxide nano thread in the electrode.
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|---|---|---|---|
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| CN101941803A (en) * | 2010-09-27 | 2011-01-12 | 彩虹集团公司 | Preparation method of titanium dioxide thin film for solar cell electrode |
| CN103030306B (en) * | 2012-12-21 | 2015-06-10 | 深圳市万业隆太阳能科技有限公司 | Conducting glass, as well as preparation method and application thereof |
| CN104112820B (en) * | 2013-04-18 | 2017-08-25 | 东北师范大学 | A kind of laminated film based on polyoxometallate |
| CN104821405B (en) * | 2015-03-12 | 2017-06-09 | 中国科学院化学研究所 | A kind of surface-assembled has titanic oxide nanometer tube modified electrode of PSII and preparation method and application |
| CN109427487B (en) * | 2017-08-31 | 2021-09-21 | 中国科学院金属研究所 | Flexible-base dye-sensitized solar cell structure and preparation method thereof |
| CN109638208B (en) * | 2018-12-25 | 2021-09-24 | 合肥国轩精密涂布材料有限责任公司 | Preparation method of organic nano composite diaphragm |
| CN110479385A (en) * | 2019-08-22 | 2019-11-22 | 浙江理工大学 | A kind of hud typed Fe that cladding size is controllable3O4The preparation method of@hydrogel nanocatalyst |
| CN113215609B (en) * | 2021-05-06 | 2022-10-21 | 福州大学 | Preparation of silver nanocluster sensitized titanium dioxide composite photo-anode for photoelectrocatalysis |
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|---|---|---|---|---|
| CN1599697A (en) * | 2001-10-30 | 2005-03-23 | 触媒化成工业株式会社 | Tubular titanium oxide particles, method for preparing the same, and use of the same |
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| CN1599697A (en) * | 2001-10-30 | 2005-03-23 | 触媒化成工业株式会社 | Tubular titanium oxide particles, method for preparing the same, and use of the same |
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